Accepted Manuscript Title: Simultaneous determination of 40 novel psychoactive stimulants in urine by liquid chromatography-high resolution mass spectrometry and library matching Author: Marta Concheiro Marisol Castaneto Robert Kronstrand Marilyn A. Huestis PII: DOI: Reference:

S0021-9673(15)00527-0 http://dx.doi.org/doi:10.1016/j.chroma.2015.04.002 CHROMA 356421

To appear in:

Journal of Chromatography A

Received date: Revised date: Accepted date:

30-11-2014 30-3-2015 1-4-2015

Please cite this article as: M. Concheiro, M. Castaneto, R. Kronstrand, M.A. Huestis, Simultaneous determination of 40 novel psychoactive stimulants in urine by liquid chromatography-high resolution mass spectrometry and library matching, Journal of Chromatography A (2015), http://dx.doi.org/10.1016/j.chroma.2015.04.002 This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

 Simultaneous novel psychoactive substances (NPS) analysis is highly challenging.

2

 NPS constantly emerge with similar or completely new chemical structures.

3

 The method quantifies 40 urinary NPS and 4 metabolites by LC-HRMS.

4

 Screening and confirmation data acquired in full scan and data dependent MS2.

5

 100 µL urine volume achieved 2.5-5 µg/L limit of quantification (LOQ).

cr

6

ip t

1

Ac ce p

te

d

M

an

us

7

Page 1 of 33

7

Simultaneous determination of 40 novel psychoactive stimulants in urine by

8

liquid chromatography-high resolution mass spectrometry and library matching

9

13 14 15 16

ip t

Chemistry and Drug Metabolism, Intramural Research Program, National Institute on

Drug Abuse, National Institutes of Health, Baltimore, MD, USA

cr

12

1

2

Currently Department of Sciences, John Jay College of Criminal Justice, City University

us

11

Marta Concheiro1,2, Marisol Castaneto1,3, Robert Kronstrand4, Marilyn A. Huestis1*

of New York, New York, NY, USA 3

Program in Toxicology, University of Maryland Baltimore, Baltimore, MD, USA

an

10

4

Department of Forensic Genetics and Forensic Toxicology, National Board of Forensic

Medicine, Linköping, Sweden Division of Drug Research, Department of Medical and

18

Health Sciences, Linköping University, Linköping, Sweden

19

d

M

17

Corresponding author

21

Professor Dr. Dr. (h.c.) Marilyn A. Huestis

22

Chief, Chemistry and Drug Metabolism

23

Biomedical Research Center (BRC)

24

National Institute on Drug Abuse, NIH

25

251 Bayview Blvd, Suite 200 Room 05A721

26

Baltimore, MD 21224

27

email: [email protected]

28

Phone: 443-740-2524

29

Fax: 443-740-2823

Ac ce p

te

20

30

Page 2 of 33

Abstract

32

The emergence of novel psychoactive substances is an ongoing challenge for analytical

33

toxicologists. Different analogs are continuously introduced in the market to circumvent

34

legislation and to enhance their pharmacological activity. Although detection of drugs in

35

blood indicates recent exposure and link intoxication to the causative agent, urine is still

36

the most preferred testing matrix in clinical and forensic settings. We developed a

37

method for the simultaneous quantification of 8 piperazines, 4 designer amphetamines

38

and 28 synthetic cathinones and 4 metabolites, in urine by liquid chromatography

39

coupled to high-resolution mass spectrometry (LC-HRMS). Data were acquired in full

40

scan and data dependent MS2 mode. Compounds were quantified by precursor ion

41

exact mass, and confirmed by product ion spectra library matching, taking into account

42

product ions’ exact mass and intensities. One-hundred µL urine was subjected to solid

43

phase cation exchange extraction (SOLA SCX). The chromatographic reverse-phase

44

separation was achieved with gradient mobile phase of 0.1% formic acid in water and in

45

acetonitrile in 20 min. The assay was linear from 2.5 or 5 to 500µg/L. Imprecision (n=15)

46

was

Simultaneous determination of 40 novel psychoactive stimulants in urine by liquid chromatography-high resolution mass spectrometry and library matching.

The emergence of novel psychoactive substances is an ongoing challenge for analytical toxicologists. Different analogs are continuously introduced in ...
517KB Sizes 2 Downloads 11 Views